WO2017185468A1 - 一种牙科用氧化锆陶瓷修复体及其制备方法 - Google Patents

一种牙科用氧化锆陶瓷修复体及其制备方法 Download PDF

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WO2017185468A1
WO2017185468A1 PCT/CN2016/084125 CN2016084125W WO2017185468A1 WO 2017185468 A1 WO2017185468 A1 WO 2017185468A1 CN 2016084125 W CN2016084125 W CN 2016084125W WO 2017185468 A1 WO2017185468 A1 WO 2017185468A1
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zirconia ceramic
powder
zirconia
dental
ceramic
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PCT/CN2016/084125
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English (en)
French (fr)
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刘谋山
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成都贝施美医疗设备有限公司
成都贝施美生物科技有限公司
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Publication of WO2017185468A1 publication Critical patent/WO2017185468A1/zh

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    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
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Definitions

  • the field of dental materials of the present invention specifically relates to a dental zirconia ceramic restoration and a preparation method thereof.
  • Tianqi is also known as Sanqi, Jinbui, Sanqishen, Blood Ginseng, Blood Ginseng, Mountain Paint, Buddha Hand Mountain Paint, Tian Paint, Tian Sanqi. It is the root of Panax notoginseng, Panax notoginseng, which is a perennial herb that grows in a humid zone. Three seven sex, slightly bitter. Panax notoginseng is conical, spindle-shaped or irregularly shaped, 1 to 6 cm long and 1 to 4 cm in diameter.
  • the surface is grayish yellow or grayish yellow, with waxy luster, stem marks on the top, knob-like protrusions around, intermittent longitudinal wrinkles and root fractures on the sides, body weight, firm texture, crushed skin and wood Often separated; cross-section gray-green, yellow-green or gray-white, with small brown resin road spots on the skin, with a slightly radial texture at the center. It is slightly fragrant, bitter and sweet. It is better to use weight, firmness, smooth surface, grayish green or yellowish green.
  • Tianqi 1, ⁇ stop bleeding: This product can not only stop bleeding, but also activating blood circulation, so blood medicine.
  • Dispersant is a surfactant that has the opposite properties of oleophilic and hydrophilic in the molecule. It can uniformly disperse solid and liquid particles of inorganic, organic pigments that are difficult to dissolve in liquids, and also prevent sedimentation and aggregation of particles, forming an amphipathic reagent required for a stable suspension. Dispersants enhance shine, prevent floating color, reduce flocculation, increase color development, increase color saturation, and increase transparency.
  • the development of oral prosthetics is inseparable from the development of oral materials and processes.
  • the denture restoration materials mainly include ceramics, resins and metal materials.
  • the traditional glass-ceramic-based and alumina-based ceramic materials are inherently insufficient in strength and brittle, and are easily broken, which limits their use in the repair of the oral cavity.
  • all-ceramic materials have become a current use due to their own good biocompatibility, corrosion resistance, dielectric properties, thermal stability and excellent aesthetic effects.
  • the all-ceramic materials commonly used for dentures are mainly alumina and zirconia.
  • Alumina has good wear resistance, but is brittle and easily broken, compared to zirconia due to its The doping action of his oxide makes it produce a stable tetragonal phase. Therefore, zirconia ceramics have high toughness, high flexural strength and high wear resistance.
  • zirconia ceramics are the most mechanically all-ceramic materials in the all-magnetic materials currently used for oral restoration, and are suitable as dental restorations.
  • the ceramic products sintered by pure zirconia ceramics are white, and the single color is difficult to meet the current personalized social needs, and the current dental zirconia restorations have hardness, antibacterial and anti-inflammatory properties, color development, etc. Need to improve, there is an urgent need to release new materials.
  • a dental zirconia ceramic restoration composed of the following raw materials by weight:
  • zirconia 5 ⁇ 25; alumina: 0.5 ⁇ 1.6;
  • ceramic powder 15 ⁇ 30; cellulose powder: 20 ⁇ 48;
  • cerium oxide 2 ⁇ 11; dispersing agent: 0.6 ⁇ 2.8;
  • water-soluble binder 1.5 ⁇ 4; Tianqi extract: 0.3 ⁇ 2.5;
  • Colorant 1.5 to 6.
  • zirconia 15; alumina: 1.1;
  • ceramic powder 23; cellulose powder: 34;
  • cerium oxide 7; dispersing agent: 1.7;
  • water soluble binder 2.7; Tianqi extract: 1.4;
  • the dispersing agent is one of sodium lauryl sulfate or methyl amyl alcohol.
  • the water-soluble binder is one of polyvinyl alcohol, polyethylene oxide or methyl cellulose.
  • the colorant is one of cerium oxide, iron chloride, cerium chloride, cerium oxide or cerium nitrate.
  • the cellulose powder has a mesh number of 600 to 800 mesh.
  • the ceramic powder has a mesh number of 700 to 800 mesh.
  • the zirconia ceramic restoration has a Vickers hardness of 14 to 15 GPa; and the zirconia ceramic restoration has a three-point bending strength of 1100 to 1200 MPa.
  • the stirring rate in step S3 is 500 to 700 rpm, and the mixture is cooled to 40 to 55 ° C after stirring.
  • the present invention has the following advantages:
  • the dental zirconia ceramic prosthesis obtained by the invention has high hardness, and a dispersant is added to the composition, which solves the problem that the all-ceramic material is fragile, the gloss is low, and the color development is poor.
  • the problem of low transparency, the addition of Tianqi extract makes the dental zirconia ceramic restoration have the functions of promoting blood circulation, relieving swelling and relieving pain, and the materials selected are widely used for human health; the dental zirconia ceramic restoration of the present invention
  • the coloring agent is added to the body composition, which satisfies the individualized social needs of modern society and has broad market prospects.
  • Example 1 A dental zirconia ceramic restoration composed of the following raw materials by weight: [0033] Zirconia: 15; Alumina: 1.1; [0034] ceramic powder: 23; cellulose powder: 34;
  • yttrium oxide 7; sodium lauryl sulfate: 1.7;
  • polyvinyl alcohol 2. 7 ; Tianqi extract: 1.4;
  • Cerium oxide 3.8.
  • the cellulose powder has a mesh number of 600 mesh; the ceramic powder has a mesh number of 700 mesh; the zirconia ceramic restoration has a Vickers hardness of 14 GPa; and the zirconia ceramic restoration
  • the three-point bending strength is 11 00 MPa.
  • Example 2 A dental zirconia ceramic restoration composed of the following raw materials by weight:
  • zirconia 5; alumina: 0.5;
  • ceramic powder 15; cellulose powder: 20;
  • cerium oxide 2; methyl pentanol: 0.6;
  • polyethylene oxide 1.5; Tianqi extract: 0.3;
  • the method for preparing a dental zirconia ceramic restoration comprising the steps of:
  • the cellulose powder has a mesh number of 800 mesh; the ceramic powder has a mesh number of 800 mesh; the zirconia ceramic restoration has a Vickers hardness of 15 GPa; and the zirconia ceramic restoration
  • the three-point bending strength is 12 00 MPa.
  • Example 3 A dental zirconia ceramic restoration consisting of the following raw materials by weight:
  • zirconia 25; alumina: 1.6;
  • ceramic powder 30; cellulose powder: 48;
  • yttrium oxide 11; sodium lauryl sulfate: 2.8;
  • methyl cellulose 4; Tianqi extract: 2.5;
  • the preparation method of the dental zirconia ceramic restoration comprises the following steps:
  • the cellulose powder has a mesh number of 700 mesh; the ceramic powder has a mesh number of 750 mesh; the zirconia ceramic restoration has a Vickers hardness of 14.5 GPa; the zirconia ceramic restoration The three-point bending strength is 1130 MPa.
  • Example 4 A dental zirconia ceramic restoration composed of the following raw materials by weight:
  • zirconia 20; alumina: 1.3;
  • ceramic powder 27; cellulose powder: 45;
  • cerium oxide 4; methyl pentanol: 0.9; [0072] polyethylene oxide: 1.7; Tianqi extract: 0.8;
  • Cerium oxide 2.1.
  • the method for preparing a dental zirconia ceramic restoration comprising the steps of:
  • the cellulose powder has a mesh number of 650 mesh; the ceramic powder has a mesh number of 720 mesh; the zirconia ceramic restoration has a Vickers hardness of 14.8 GPa; the zirconia ceramic restoration The three-point bending strength is 1170 MPa.
  • Example 5 A dental zirconia ceramic restoration consisting of the following raw materials by weight:
  • zirconia 9; alumina: 0.7;
  • ceramic powder 17; cellulose powder: 26;
  • cerium oxide 9; sodium lauryl sulfate: 2.6;
  • methylcellulose 3.5; Tianqi extract: 2.2;
  • the method for preparing a dental zirconia ceramic restoration comprising the steps of:
  • the cellulose powder has a mesh number of 770 mesh; the ceramic powder has a mesh number of 730 mesh; the oxidized ceramic restoration has a Vickers hardness of 14.2 GPa; and the zirconia ceramic restoration
  • the three-point bending strength is 1120 MPa.
  • Example 6 A dental zirconia ceramic restoration composed of the following raw materials by weight:
  • zirconia 13; alumina: 1.1;
  • ceramic powder 22; cellulose powder: 35;
  • cerium oxide 8; methyl pentanol: 1.6;
  • polyvinyl alcohol 3.8; Tianqi extract: 2.2;
  • Cerium oxide 4.8.
  • the preparation method of the dental zirconia ceramic prosthesis comprises the following steps:
  • the cellulose powder has a mesh number of 700 mesh; the ceramic powder has a mesh number of 760 mesh; the oxidized ceramic restoration has a Vickers hardness of 14.6 GPa; and the zirconia ceramic restoration
  • the three-point bending strength is 1150 MPa.

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  • Ceramic Engineering (AREA)
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  • Oral & Maxillofacial Surgery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Composite Materials (AREA)
  • Plastic & Reconstructive Surgery (AREA)
  • Epidemiology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Dental Preparations (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

一种牙科用氧化锆陶瓷修复体及其制备方法，所述牙科用氧化锆陶瓷修复体由氧化锆、氧化铝、陶瓷粉、纤维素粉、氧化钇、分散剂、水溶性粘结剂、田七提取液和着色剂组成。牙科用氧化锆陶瓷修复体的制备方法包括称量、研磨、搅拌和干燥。得到的牙科用氧化锆陶瓷修复体具有较高的硬度，且选用的材料来源广，对人体健康；该牙科用氧化锆陶瓷修复体的成分中加入了着色剂，满足了现代社会个性化的社会需求，具有广阔的前景；该牙科用氧化锆陶瓷修复体的制备方法操作简单、制备方便、成本低、适用于工业化大规模生产。

Description

说明书 发明名称：一种牙科用氧化锆陶瓷修复体及其制备方法 技术领域
[0001] 本发明牙科材料领域， 具体涉及一种牙科用氧化锆陶瓷修复体及其制备方法。
背景技术
[0002] 田七又名三七、 金不换、 三七参、 血参、 血参、 山漆、 佛手山漆、 田漆、 田三 七。 为五加科植物三七的根， 三七， 属多年生草本植物， 生长在潮湿地带。 三 七性温， 微苦。 三七根呈类圆锥形， 纺锤形或不规则块状， 长 1至 6厘米， 直径 1 至 4厘米。 表面灰黄色或灰黄棕色， 具蜡样光泽， 顶端有茎痕， 周围有瘤状突起 ， 侧面有断续的纵皱及支根断痕， 体重， 质坚实， 击碎后皮部与木部常分离； 横断面灰绿色， 黄绿色或灰白色， 皮部有细小棕色树脂道斑点， 中心微显放射 状纹理。 气微， 味苦而后甜。 以体重、 质坚、 表面光滑、 断面灰绿色或黄绿色 者为佳。 田七的功效： 1、 祛瘀止血： 本品既能止血， 又能活血散瘀， 为止血良 药。 可用于治疗各种出血证； 2、 消肿止痛： 治疗跌打瘀肿疼痛、 瘀血内阻所致 的胸腹及关节疼痛， 能活血化瘀消肿； 3、 三七有比较好的降低胆固醇， 降低甘 油三脂的作用。 分散剂 （Dispersant) 是一种在分子内同吋具有亲油性和亲水 性两种相反性质的界面活性剂。 可均一分散那些难于溶解于液体的无机， 有机 颜料的固体及液体颗粒， 同吋也能防止颗粒的沉降和凝聚， 形成安定悬浮液所 需的两亲性试剂。 分散剂可以提升光泽、 防止浮色发花、 减少絮凝、 增加展色 性， 增加颜色饱和度、 增加透明度。
[0003] 口腔修复的发展与口腔材料和工艺的发展密不可分， 义齿修复材料主要有陶瓷 、 树脂和金属材料。 而传统的玻璃陶瓷基和氧化铝基的陶瓷材料本身强度不足 且脆性较大， 易破裂， 限制了其在口腔的修复中的使用。
[0004] 随着当前口腔修复技术的飞速发展， 全瓷材料凭借着自身良好的生物相容性、 耐腐蚀性、 介电性、 热稳定性以及优良的美学效果等一系列特质， 成为目前使 用最广泛的口腔修复材料。 通常制作义齿的全瓷材料主要有氧化铝和氧化锆， 氧化铝具有良好的耐磨性能， 但是脆性较大， 易破裂， 相比之下氧化锆由于其 他氧化物的参杂作用使其产生稳定的四方晶相， 因此， 氧化锆陶瓷具有高韧性 、 高抗弯强度和高耐磨性。 因此， 氧化锆陶瓷是目前用于口腔修复的全磁材料 中机械性能最好的全瓷材料， 适宜作为牙科修复体。 但是纯氧化锆陶瓷烧结出 来的陶瓷产品是白色的， 单一的这种颜色难以满足现在个性化的社会需求， 且 目前的牙科氧化锆修复体在硬度、 抗菌消炎及其光泽度、 展色性等上需要提高 ， 急需幵发新的材料。
技术问题
[0005] 本发明的目的在于克服现有技术的缺点， 提供一种牙科用氧化锆陶瓷修复体。
问题的解决方案
技术解决方案
[0006] 本发明的目的通过以下技术方案来实现： 一种牙科用氧化锆陶瓷修复体， 它由 下述重量份的原料组成：
[0007] 氧化锆： 5〜25； 氧化铝： 0.5〜1.6；
[0008] 陶瓷粉： 15〜30； 纤维素粉： 20〜48；
[0009] 氧化钇： 2〜11； 分散剂： 0.6〜2.8；
[0010] 水溶性粘结剂： 1.5〜4； 田七提取液： 0.3〜2.5；
[0011] 着色剂： 1.5〜6。
[0012] 优选地， 它由下述重量份的原料组成：
[0013] 氧化锆： 15; 氧化铝： 1.1 ;
[0014] 陶瓷粉： 23; 纤维素粉： 34;
[0015] 氧化钇： 7; 分散剂： 1.7;
[0016] 水溶性粘结剂： 2.7; 田七提取液： 1.4;
[0017] 着色剂： 3.8。
[0018] 进一步地， 所述分散剂为十二烷基硫酸钠或甲基戊醇中的一种。
[0019] 进一步地， 所述水溶性粘结剂为聚乙烯醇、 聚环氧乙烷或甲基纤维素中的一 种。
[0020] 进一步地， 所述着色剂为氧化铈、 氯化铁、 氯化铒、 氧化镨或硝酸镨中的一 种。 [0021] 上述牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0022] S1.称量： 按上述配方比例称取各原料， 备用；
[0023] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 分散剂和着色剂投入球磨机 中进行研磨， 所述研磨的吋间为 1.5〜3.5h， 得研磨粉料混合物；
[0024] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和水溶 性粘结剂， 搅拌 30〜50min冷却后加入田七提取液， 搅拌均匀得搅拌混合物；
[0025] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2〜3h， 即制得牙科用氧化 锆陶瓷修复体。
[0026] 进一步地， 所述纤维素粉的目数为 600〜800目。
[0027] 进一步地， 所述陶瓷粉的目数为 700〜800目。
[0028] 进一步地， 所述氧化锆陶瓷修复体的维氏硬度达到 14〜15GPa; 所述氧化锆陶 瓷修复体的三点抗弯强度为 1100〜1200MPa。
[0029] 进一步地， 步骤 S3中所述搅拌的速率为 500〜700rpm， 搅拌后冷却至 40〜55°C 发明的有益效果
有益效果
[0030] 本发明具有以下优点： 采用本发明得到的牙科用氧化锆陶瓷修复体具有较高的 硬度， 其成分中加入了分散剂， 解决了全瓷材料易碎、 光泽度低、 展色性差、 透明度低的问题， 加入了田七提取液使得牙科用氧化锆陶瓷修复体具有活血化 瘀、 消肿止痛的作用， 且选用的材料来源广， 对人体健康； 本发明牙科用氧化 锆陶瓷修复体成分中加入了着色剂， 满足了现代社会个性化的社会需求， 具有 广阔的市场前景。
实施该发明的最佳实施例
本发明的最佳实施方式
[0031] 下面结合实施例对本发明做进一步的描述， 本发明的保护范围不局限于以下所 述。
[0032] 实施例 1: 一种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成： [0033] 氧化锆： 15; 氧化铝： 1.1 ; [0034] 陶瓷粉： 23; 纤维素粉： 34;
[0035] 氧化钇： 7; 十二烷基硫酸钠： 1.7;
[0036] 聚乙烯醇： 2.7； 田七提取液： 1.4;
[0037] 氧化铈： 3.8。
[0038] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0039] S1.称量： 按上述配方比例称取各原料， 备用；
[0040] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 十二烷基硫酸钠和氧化铈投 入球磨机中进行研磨， 所述研磨的吋间为 1.5h， 得研磨粉料混合物；
[0041] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和聚乙 烯醇， 以 500rpm的速度搅拌 30min冷却至 40°C后加入田七提取液， 搅拌均匀得搅 拌混合物；
[0042] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2h， 即制得牙科用氧化锆 陶瓷修复体。
[0043] 其中， 所述纤维素粉的目数为 600目； 所述陶瓷粉的目数为 700目； 所述氧化锆 陶瓷修复体的维氏硬度达到 14GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 11 00MPa。
[0044] 实施例 2: —种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成：
[0045] 氧化锆： 5; 氧化铝： 0.5;
[0046] 陶瓷粉： 15; 纤维素粉： 20;
[0047] 氧化钇： 2; 甲基戊醇： 0.6;
[0048] 聚环氧乙烷： 1.5; 田七提取液： 0.3;
[0049] 氯化铁： 1.5。
[0050] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0051] S1.称量： 按上述配方比例称取各原料， 备用；
[0052] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 甲基戊醇和氯化铁投入球磨 机中进行研磨， 所述研磨的吋间为 3.5h， 得研磨粉料混合物；
[0053] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和聚环 氧乙烷， 以 700rpm的速度搅拌 50min冷却至 55。C后加入田七提取液， 搅拌均匀得 搅拌混合物；
[0054] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 3h， 即制得牙科用氧化锆 陶瓷修复体。
[0055] 其中， 所述纤维素粉的目数为 800目； 所述陶瓷粉的目数为 800目； 所述氧化锆 陶瓷修复体的维氏硬度达到 15GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 12 00MPa。
[0056] 实施例 3: —种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成：
[0057] 氧化锆： 25 ; 氧化铝： 1.6;
[0058] 陶瓷粉： 30; 纤维素粉： 48 ;
[0059] 氧化钇： 11 ; 十二烷基硫酸钠： 2.8 ;
[0060] 甲基纤维素： 4; 田七提取液： 2.5 ;
[0061] 氯化铒： 6。
[0062] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0063] S1.称量： 按上述配方比例称取各原料， 备用；
[0064] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 十二烷基硫酸钠和氯化铒投 入球磨机中进行研磨， 所述研磨的吋间为 2.5h， 得研磨粉料混合物；
[0065] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和甲基 纤维素， 以 600rpm的速度搅拌 40min冷却至 48°C后加入田七提取液， 搅拌均匀得 搅拌混合物；
[0066] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2.5h， 即制得牙科用氧化 锆陶瓷修复体。
[0067] 其中， 所述纤维素粉的目数为 700目； 所述陶瓷粉的目数为 750目； 所述氧化锆 陶瓷修复体的维氏硬度达到 14.5GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 1130MPa。
[0068] 实施例 4: 一种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成：
[0069] 氧化锆： 20; 氧化铝： 1.3 ;
[0070] 陶瓷粉： 27 ; 纤维素粉： 45 ;
[0071] 氧化钇： 4; 甲基戊醇： 0.9; [0072] 聚环氧乙烷： 1.7; 田七提取液： 0.8;
[0073] 氧化镨： 2.1。
[0074] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0075] S1.称量： 按上述配方比例称取各原料， 备用；
[0076] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 甲基戊醇和氧化镨投入球磨 机中进行研磨， 所述研磨的吋间为 2h， 得研磨粉料混合物；
[0077] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和聚环 氧乙烷， 以 550rpm的速度搅拌 35min冷却至 42。C后加入田七提取液， 搅拌均匀得 搅拌混合物；
[0078] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2.2h， 即制得牙科用氧化 锆陶瓷修复体。
[0079] 其中， 所述纤维素粉的目数为 650目； 所述陶瓷粉的目数为 720目； 所述氧化锆 陶瓷修复体的维氏硬度达到 14.8GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 1170MPa。
[0080] 实施例 5: —种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成：
[0081] 氧化锆： 9; 氧化铝： 0.7;
[0082] 陶瓷粉： 17; 纤维素粉： 26;
[0083] 氧化钇： 9; 十二烷基硫酸钠： 2.6;
[0084] 甲基纤维素： 3.5; 田七提取液： 2.2;
[0085] 硝酸镨： 5.2。
[0086] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0087] S1.称量： 按上述配方比例称取各原料， 备用；
[0088] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 十二烷基硫酸钠和硝酸镨投 入球磨机中进行研磨， 所述研磨的吋间为 3h， 得研磨粉料混合物；
[0089] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和甲基 纤维素， 以 680rpm的速度搅拌 45min冷却至 52°C后加入田七提取液， 搅拌均匀得 搅拌混合物；
[0090] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 3h， 即制得牙科用氧化锆 陶瓷修复体。
[0091] 其中， 所述纤维素粉的目数为 770目； 所述陶瓷粉的目数为 730目； 所述氧化 陶瓷修复体的维氏硬度达到 14.2GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 1120MPa。
[0092] 实施例 6: —种牙科用氧化锆陶瓷修复体， 它由下述重量份的原料组成：
[0093] 氧化锆： 13; 氧化铝： 1.1 ;
[0094] 陶瓷粉： 22; 纤维素粉： 35;
[0095] 氧化钇： 8; 甲基戊醇： 1.6;
[0096] 聚乙烯醇： 3.8; 田七提取液： 2.2;
[0097] 氧化镨： 4.8。
[0098] 该牙科用氧化锆陶瓷修复体的制备方法， 它包括以下步骤：
[0099] S1.称量： 按上述配方比例称取各原料， 备用；
[0100] S2.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 甲基戊醇和氧化镨投入球磨 机中进行研磨， 所述研磨的吋间为 2h， 得研磨粉料混合物；
[0101] S3.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素粉和聚乙 烯醇， 以 650rpm的速度搅拌 37min冷却至 45°C后加入田七提取液， 搅拌均匀得搅 拌混合物；
[0102] S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2h， 即制得牙科用氧化锆 陶瓷修复体。
[0103] 其中， 所述纤维素粉的目数为 700目； 所述陶瓷粉的目数为 760目； 所述氧化 陶瓷修复体的维氏硬度达到 14.6GPa; 所述氧化锆陶瓷修复体的三点抗弯强度为 1150MPa。

Claims

权利要求书
[权利要求 1] 一种牙科用氧化锆陶瓷修复体， 其特征在于， 它由下述重量份的原料 组成：
氧化锆： 5〜25； 氧化铝： 0.5〜1.6；
陶瓷粉： 15〜30； 纤维素粉： 20〜48；
氧化钇： 2〜11； 分散剂： 0.6〜2.8；
水溶性粘结剂： 1.5〜4； 田七提取液： 0.3〜2.5；
着色剂： 1.5〜6。
[权利要求 2] 如权利要求 1所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 它 由下述重量份的原料组成：
氧化锆： 15; 氧化铝： 1.1 ;
陶瓷粉： 23; 纤维素粉： 34;
氧化钇： 7; 分散剂： 1.7;
水溶性粘结剂： 2.7; 田七提取液： 1.4;
着色剂： 3.8。
[权利要求 3] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述分散剂为十二烷基硫酸钠或甲基戊醇中的一种。
[权利要求 4] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述水溶性粘结剂为聚乙烯醇、 聚环氧乙烷或甲基纤维素中的一种。
[权利要求 5] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述着色剂为氧化铈、 氯化铁、 氯化铒、 氧化镨或硝酸镨中的一种。
[权利要求 6] 如权利要求 1〜5中任一权利要求所述的一种牙科用氧化锆陶瓷修复体 的制备方法， 其特征在于， 它包括以下步骤：
51.称量： 按上述配方比例称取各原料， 备用；
52.研磨： 将氧化锆、 氧化铝、 陶瓷粉、 氧化钇、 分散剂和着色剂投 入球磨机中进行研磨， 所述研磨的吋间为 1.5〜3.5h， 得研磨粉料混合 物；
53.搅拌： 将研磨粉料混合物中加入到坩埚中， 加热后再加入纤维素 粉和水溶性粘结剂， 搅拌 30〜50min冷却后加入田七提取液， 搅拌均 匀得搅拌混合物；
S4.干燥： 将上述搅拌混合物倒入模具中， 真空干燥 2〜3h， 即制得牙 科用氧化锆陶瓷修复体。
[权利要求 7] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述纤维素粉的目数为 600〜800目。
[权利要求 8] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述陶瓷粉的目数为 700〜800目。
[权利要求 9] 如权利要求 1或 2所述的一种牙科用氧化锆陶瓷修复体， 其特征在于， 所述氧化锆陶瓷修复体的维氏硬度达到 14〜15GPa; 所述氧化锆陶瓷 修复体的三点抗弯强度为 1100〜1200MPa。
[权利要求 10] 如权利要求 6所述的一种牙科用氧化锆陶瓷修复体的制备方法， 其特 征在于， 步骤 S3中所述搅拌的速率为 500〜700rpm， 搅拌后冷却至 40
〜55。C。
PCT/CN2016/084125 2016-04-29 2016-05-31 一种牙科用氧化锆陶瓷修复体及其制备方法 WO2017185468A1 (zh)

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